Solidified liquid fuel and process for its production



Patented Apr. 18, 1950 SOLIDIFIED LIQUID FUEL AND PROCESS FOR, ITS PRODUCTION Harry N. Holmes, Oberlin, Ohio, assignor to Sterno, Inc., ,New'York, N. Y., a corporation of New York No Drawing. Application August 14, 1948,

, Serial No. 44,391

The invention relates to a process for the production of a solidified liquid fuel and to the product thus obtained. More particularly, it pertains to a nitrocellulose-alcogel in the form of discrete portions having a protective coating, or

envelope and includes correlated improvements and discoveries whereby the qualities thereof are enhanced.

It is an object of the invention to provide a process in accordance with which shrinkage and syneresis of discrete portions of a nitrocellulosealcogel may be substantially eliminated.

A further object of the invention is to provide a procedure in accordance with which a nitrocellulose-alcogel may be produced of which dis crete portions thereof are provided with a coating, or envelope that tends to maintain the nitrocellulose-alcogel in its original condition.

check, or break away, and substantially obviates shrinkage and syneresis.

A particular object of the invention is the provision, as an article of manufacture, of a nitroceIlulose-alcogel, in the form of discrete portions enveloped in a composition containing a nitrocellulose and a glyceryl phthalate.

Other objects of the invention will in part be obvious and will in part appear hereinafter.

The invention accordingly comprises the several steps, and the relation of one or more of such steps with respect to each of the others, and the composition possessing the features, and properties, which are exemplified in the following detailed disclosure, and the scope of the invention will be indicated in the claims.

In the practise of the invention, a solidified liquid fuel may be produced through solidification of a liquid fuel by means of a gel-forming substance, e. g., dissolving a nitrocellulose in a lower aliphatic alcohol and solidifying by the addition thereto of a non-solvent for the nitrocellulose, and with respect to which, discrete portions thereof are coated with a collodion composition containing a nitrocellulose, and more particularly, a nitrocellulose containing from about 10.5% to about 12% of nitrogen, a water- 6 "Claims. (Cl. 44-7) soluble alcohol as a solvent therefor, which suitably maybe a denatured ethyl alcohol, and a glyceryl phthalate.

It may be desirable to include a diluent in the coating composition. When such is included, its character and the amount thereof will depend upon the constituents present in the coating composition. The diluent may be a further quantity of a diluted alcohol, a relatively low boiling petroleum distillate, as a naphtha, petroleum ether, and the like, or a low boiling aromatic hydrocarbon, as benzene and toluene. Moreover, the glyceryl phthalate may in one modification, be a water-white, solid resin having a specific gravity of about 1.29, a saponification value of 605-615, an acid value of 300-315, and a softening point at about 67 C., and in another modification, a soft solid of straw color having a specific gravity of about 1.29, a saponification value of 325-335 and an acid value of 3050.

It has been found to be advisable to have an amount of a glyceryl phthalate, which ranges from about 0.25 part to about 1.5 parts thereof to about 10 parts of a collodion composition, e. g., a nitrocellulose solution, and satisfactory results flow from the utilization of 0.75 part. Also, it has been found that with a lesser amount of the glyceryl phthalate, a satisfactory covering of the fuel is not obtained, and that when a larger amount is employed, the coating tends to be rather tacky, and hence undesirable.

solidified liquid fuels may contain a lower aliphatic alcohol and mixtures of such alcohols, as methyl, ethyl, and isoand normal propyl alcohols. The collodion composition to which the resin is added may be prepared by taking a nitrocellulose, which maybe a mixture of triand tetranitrocellulose, about 40 grams and dis-- solving it in ether about 750 c. c. and ethanol about 250 c. c. It will be realized that other collodion compositions may be employed, as solutions of a nitrocellulose in the lower aliphatic alcohols, e. g., methanol and ethanol and admixtures thereof and such a general type collodion and its preparation are set forth in Patent 1,934,860.

As an illustrative embodiment of a manner in which the invention may be pract ced, the following examples are given.

Example 1 A coating composition may be prepared by dissolving 0.5 gram of a glyceryl phthalate in about 10 c. 0. ethanol, which may be denatured, and

Example 2 1 gram of a glyceryl phthalate is dissolved in about c. c. of ethanol. The solution so obtained is mixed with about 10 c. c. of the collodion of Example 1. When this composition was utilized, it was found that the film, or envelope, did not break or'crack, covered well and was only slightly tacky.

Example 3 With 10 c. c. of the collodion of Example 1, there was admixed a solution prepared by dissolving 0.25 gram of a glyceryl phthalate in about 10 c. c. of ethanol. The film, or envelope, formed after drying evidenced rather material shrinkage and was therefore not as well adapted for the formation of an envelope for cubes of a solidified fuel, e. g., a solid alcohol.

Example 4 A highly effective coating composition may be produced by dissolving 3 grams of a water-white, solid glyceryl phthalate having a specific gravity of about 1.29 and a softening point at about 67 C. in about 25 c. c. of ethanol and then adding this solution to 40 c. c. of a collodion as defined in Example 1.

This composition may be applied to cubes of a nitrocellulose-alcogel, which contains a nitrocellulose, denatured alcohol, water and a coloring material, by dipping or immersion. The coated cubes are then permitted to dry by placing on a wet glass surface and allowing to stand in the air for a period of time sufiicient to accomplish an efiective removal of solvent. The film, so produced gives full coverage of the cube; is nontacky, transparent and readily combustible; exhibits substantially no shrinkage or warpage and after a period of several months, there was not any syneresis, or bleeding, of liquid from the nitrocellulose-alcogel cubes.

The foregoing procedure leads to the production of a nitrocellulose-alcogel, in the form of discrete portions, which may be cubes or tablets of a convenient size, that even after an extended period of time does not show any substantial shrinkage, or any material syneresis.

The usual manner in which the enveloped portions are marketed is in substantially airtight containers from which the portions may be removed as desired.

It may be added that the coating should possess the following characteristics; substantial resistance to the free fiow of liquid ethyl and methyl alcohols; ignite easily and burn readily without smoke or odor; should not detract from the appearance of the discrete portion, as a cube; should coat the cube with a continuous film, should not shrink or swell on standing, and should dry entirely at room tem oerature.

Since certain changes in carrying out the above method and certain modifications in the composition which embody the invention may be made without departing from its scope, it is intended that all matter contained in the above description shall be interpreted as illustrative and not in a limiting sense.

It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described, and all statements of the scope of the invention which, as a matter of language, might be said to fall therebetween.

Having described my invention, what I claim as new and desire to secure by Letters Patent is:

1. In a process for the production of a solidified fuel which includes dissolving a nitrocellulose in a lower aliphatic alcohol and solidifying by the addition thereto of a non-solvent for the nitrocellulose, the improvement which comprises coating discrete portions of a nitrocellulose-alcogel with a composition containing a nitrocellulose having a nitrogen content from about 10.5 to about 12%, a water-soluble alcohol as a solvent therefor, and a glyceryl phthalate in an amount from about 0.25 part to about 1.5 parts of the glyceryl phthalate to about 10 parts of the nitrocellulose solution, and subsequently drying said coating.

2. In a process for the production of a solidified fuel which includes dissolving a nitrocellulose in --a lower aliphatic alcohol and solidifying by the addition thereto of a non-solvent for the nitrocellulose, the improvement which comprises coating discrete portions of a nitrocellulose-alcogel with a composition containing a nitrocellulose, a water-soluble alcohol as a solvent therefor and a glyceryl phthalate in an amount from about 0.25 part to about 1.5 parts of the glyceryl phthalate to about 10 parts of the nitrocellulose solution, and subsequently drying said coating.

3. In a process for the production ofa solidified fuel which includes dissolving a nitrocellulose in a lower aliphatic alcohol and solidifying by the addition thereto of a non-solvent for the nitrocellulose, the improvement which comprises coating discrete portions of a nitrocellulose-alcogel with a composition containing a nitrocellulose containing from about 10.5% to about 12% of nitrogen, a water-soluble alcohol as a solvent therefor and a glyceryl phthalate in an amount of about 0.75 part ofthe glyceryl phthalate to about 10 parts of the nitrocellulose solution, and subsequently drying said coating composition.

4. As an article of manufacture, a nitrocellulose-alcogel in the form of discrete portions enveloped in a composition containing a nitrocellulose and a glyceryl phthalate, the glyceryl phthalate being in an amount from about 0.25 part to about 1.5 parts to about 10 parts of the nitrocellulose coating composition.

5. As an article of manufacture, a nitrocellulose-alcogel in the form of discrete portions enveloped in a composition containing a nitrocellulose having a nitrogen content from about 10.5% to about 12% and a glyceryl phthalate, the glyceryl phthalate being in an amount from about 0.25 part to about 1.5 parts to about 10 parts of the nitrocellulose composition.

6. As an article of manufacture, a nitrocellulose-alcogel in the form of discrete portions enveloped in a composition containing a nitrocellulose having a nitrogen content from about 10.5% to about 12% and a glyceryl phthalate, which is a water-white solid having a specific gravity of about 1.29 and a softening point of about 67 C., the glyceryl phthalate being present in an amount of about 0.75 part to about 10 parts of the nitrocellulose composition.

HARRY N. HOLMES.

No references cited. 

1. IN A PROCESS FOR THE PRODUCTION OF A SOLIDIFIED FUEL WHICH INCLUDES DISSOLVING A NITROCELLULOSE IN A LOWER ALIPHATIC ALCOHOL AND SOLIDIFYING BY THE ADDITION THERETO OF A NON-SOLVENT FOR THE NITROCELLULOSE, THE IMPROVEMENT WHICH COMPRISES COATING DISCRETE PORTIONS OF A NITROCELLULOSE-ALCOGEL WITH A COMPOSITION CONTAINING A NITROCELLULOSE HAVING A NITROGEN CONTENT FROM ABOUT 10.5 TO ABOUT 12%, A WATER-SOLUBLE ALCOHOL AS A SOLVENT THEREFOR, AND A GLYCERYL PHTHALATE IN AN AMOUNT FROM ABOUT 0.25 PART TO ABOUT 1.5 PARTS OF THE GLYCERYL PHTHALATE TO ABOUT 10 PARTS OF THE NITROCELLULOSE SOLUTION, AND SUBSEQUENTLY DRYING SAID COATING. 